Method and apparatus of refining hydrocarbon oil



septjz-L 1937;l

METHOD AND APPARATUS vOF REFININGHYDROCARBON OIL Filed Feb. 5, -1935 2V sheets-sheet 1 JNVENTOR.. l

ATTORNEY Pavten'ted Sept. 21, 1937 v UNITED STATES PATENT OFFICE METHOD Anm-APPARATUS or' nEFlNr-NG nYDRooAnBoN on.

Walter J. Podbelnak, Chicago, Ill. Application February 45, 1935, Serial No.- 5,059 1s claims. (ci. 19e-4o) The present invention relates to improvements in processes and apparatus for effecting countercurrent contact of fluids and more particularly of partly or wholly immiscible liquids of different such as naphtha, lubricating oil, or the like, and sulphuric acids has been referred to. It will' be understood, however, that such references are for the purpose of illustration and are not to be 5 densities. It is in part a continuation of my regarded as limitations upon the processes and 5 prior' applications, Serial No. 476,190, filed August apparatus described. f

18, 1930, Patent No. 2,004,011,`June 4, 1935, and Referring to the drawings, the numeral I0 Serial No. 628,152, filed August 10, 1932, Patent indicates a suitable supporting frame of cast iron No. 2,003,308, June 4, 1935. The invention will or other material to which is attached a casing II :o be understood from the following description, of generally cylindrical form,in the form illus- 10 illustrated by the accompanying drawings, in trated in the drawings, with its axis horizontal. Which- A As shown-the casing II may be cast integrally Figure 1 ls an elevation partly in section' of -a lwith the frame I0 although, obviously, the casing i device suitable for carrying out the invention; and frame may be formed separatelyand secured I5 Fig. 2 is a vertical sectional view through the. together in any suitable manner. Within the 15 20 modified form of surface ofthe rotor passage of a suitable stuffing box or sealing device I4, formed 20 the device of Figs. 1 and 2. as an extension of onewall of the casing I I. The In my prior applications hereinbeforereferred hollow shaft I3 extends throughand is mounted to, there are shown devices and processes wherein in a bearing I5 at the opposite end of the frame I0 uids of different densities are brought. into inti- A in the casing II, the bearing I5 likewise being 25 mate contact with each other and wherein the provided with suitable packing or sealing devices.' 25 impelling action of centrifugal force is employed The hollow shaft I3 then opens'into a chamber I6, to secure' eifective contact of the fluids and the purpose of which will be more fully hereinvelocities, capacities and completeness of inter-' after described. At a suitable point, for example, action to an extent not hitherto possible.` In between the bearings and seals I4 and I5,apulley 3o accordance with the present invention I am en- I1 is mounted on the hollow shaft I3, by means 30 abled to. secure't effective counter-current action 0f which the latter, together with-the rotor I2, between liquids of different specific gravities, such may be rotated at any desired speed. liquids `being wholly or partly immiscible. As will Upon the rear wall or plate I8 of the rotor. I2 be readily apparent, the apparatus herein dethere is mounted a spirally-wound'strip or sheet :i5 scribed may also beemployed in securing counter- I9. The space between thev windings of this strip 35 f current contact between vapors and liquids. forms a. spiral passageway, designated by the The processes and apparatus of the present innumeral 20, which is open at its inner end, the vention may be employed in manytypes of operalatter being at approximately the -axis of rotation tions in which it is desired to secure effective of the rotor I2. At the outer circumference of 4o' contact of liquids, For example, it may be. emthe rotor there is secured to the latter the cylin 40A ployed where the liquids are intended to4 react drical retainer 2l, suitably formed as a wall memupon each other or upon constituents present in ber provided at intervals -with openings 22,

one another, for example, as in the reningf of through. which liquid contained in the casing II oils with sulphuric'acid,valkaline solutions, and may communicate with the interior of the rotor 45 the` like. It may also. be employed in solvent I2 and with the outer end of theespiral-passage 20. 45

extraction processes, such as the extractionv of Inv the form shown, the spiral passage 20 is of Voils of various typesl withl relatively immiscible generally rectangular cross-section. solvents such as liquid sulphur dioxide, nitro- The front-wall or face of the rotor I2 is formed benzene, phenol,and the like. It may also beused by aremovable plate 23 which is provided with 5J- toeiect the dehydration of .organic substances grooves 24, cut in theform ofy a spiral and into 50 and for other purposes wherein interaction' or which the free ends of the spiral web or coil lISI reaction between immiscible liquids isv desired. are closely fitted, .the plate 23 thereby closing For purposes of illustration, in theaccompanying the lspiral passage 2li.l 1f desired, a rubber or 5 description of the apparatus shown in the draw.- other suitable packing, as indicated at 25, may '55 apparatus of Fig'. 1 on the section line 2; Fig. 3 is a detailed sectional view through a portion of the rotor, and

Fig. 4 is a detailed sectional view showing a ings, interaction between a petroleum oil fraction casingl I I there is provided a rotating element or* rotor I2', the construction of which will be more fully hereinafter described. The rotor I2 is attached to a hollow shaft I3, which passes through be provided in the spiral groove 24 inthe removable plate 23, if necessary to secure a tight seal. The plate 23 may be secured to the rotor I2 by any suitable means, for example, by screws as indicated at 26.

The outer face of the casingv II is closed by a removable plate 21, which may be secured to the casing by any suitable means, for example, by the hinged bolts 28. The casing II is likewise provided with a suitable inlet 29 to which may be connected the supply line for the oil or other like liquid to be supplied to the apparatus. The casing II is also provided, preferably at its lowermost point, with a discharge conduit 30,

through which discharge of liquid froml the apparatus is eilected. As shown in the form illustrated, the discharge conduit 30 communicates liquid, for example, sulphuric acid and sludge with an enlarged chamber 3| in which separation of heavy liquid may be effected from the lighter from oil. This chamber 3| is provided at its bottom with an outlet line 32 closed by a valve 33. Within the enlarged chamber 3| there is provided a iioat 34 which, through a suitable mechanism, such as the compressed air control valve 35 and the air driven piston 36, operates to open the valve 33 and permit the discharge of separated heavy liquid orA acid from the enlarged chamber 3| when the level of the separated heavy liquid in the latter exceeds a predetermined point.

As has been indicated hereinbefore, the interior of the spiral passage 20 communicates with the central opening in the hollow shaft I3, the opening inthe hollow shaft in turn communicating with the chamber i6. The latter is provided with an outlet connection 31, through which lighter liquid or oil may be discharged from the system. A stationary pipe 38 passes through the outer wall of the chamber IB and through the central opening of the hollow shaft I3, terminating within the innermost turn of the spiral passage 20 and being provided there with slots as indicated at 39 to permit the feed of heavy liquid or acidA into the innermost portion of the spiral passage. At its outer end fit the pipe 38 is provided with a connection through which the acid or other lheavier liquid may be supplied.v

In operations involving interaction between liquids, for example, the treatment of a heavy hydrocarbon oil fraction such as a lubricant oil having a.. specific gravity in the order of 0.8 with sulphuric acid such as is usually employed having a specific gravity in the order of 1.6 to 1.8,

-difiiculties have hitherto been encountered by reason of the density of oil, the density of sludge formation and the character of the sludge formed, the diiilculty of settling the mixture to secure separation of the oil, sludge and acid after treatment and the tendency of the mixture to emulsify. I n subsequent washing an alkali treatment of the acid treated oil, difiiculties are likewise encountered in settling, in the tendency of the mixture to emulsify, in the viscosity of the oil and in the relatively smaller differences in the specific gravityof the oil and the washing liquid. By employing the process of the present invention, these difiiculties are substantially entirely avoided and at the same time a continuous operation is secured with a prolonged vand effective contact of the oil and the acid or washingv liquid.

vTo illustrate the operation of the apparatus and process, for example, in the treatment of oil 0f the character hereinbefore referred to with sulphuric acid, the oil to be treated is fed under a suitable pressure to the casing containing the rotor I2 through the connection 29. 'I'he treating liquid or acid is fed through the connection 40 to the stationary pipe 38 and reaches the innermost turn of the spiral passage 20, passing through the slotted openings 39 in the end of the pipe.

The oil and the acid being supplied in the proper proportions, the rotor is rotated at a suitable speed to secure an vadequate centrifugal force acting upon the liquids present to cause a continuous outward movement of the heavy liquid or acid. through the spiral passage 20. Inv passing through the spiral passage, the heavy liquid distributes itself inv a film or layer upon the inner surface of the outer wall of the turns of the spiral passage-way. 'I'he difference in density between the acid or heavier liquid and the oil or lighter liquid is effective, under the centrifugal force supplied, to force the acid outwardly through the spiral passage, while the oil or lighter liquid is forced into the casing under such applied pressure as to cause it to travel in the reverse direction'through the spiral passage. 'I'he direction of rotation of the rotor may be in either direction and is preferably as shown in Fig. 2, in the direction of a decreasing radius of the spiral passage-way.

The acid or any accompanying sludge or product of treatment is discharged at the outside of the passage-way through thelopenings 22 in the outer wall 2| of the rotor and enters the casing pressure under which it is supplied to the system.

reaches the innermost turn of the spiral passage and passes out through the opening in the hollow shaft I3 aroundthe -pipe 3l and discharges 4into the chamber in thecasing I8, from which it may be withdrawn through the connection 31. If desired, another removal pipe or drain pipe 42 may be provided at the lowermost point in the casing I6, and a suitable gauge column 43. may be provided to indicate the level of liquid therein.

In the form shown in the drawings, the spiral passage-way 20 is shown as of constant pitch throughout and therebythe enective or tangential component of the centrifugal force, acting upon the liquids present is substantially constant through the travel of the liquid. If desired-the pitch of the spiral passage 20 may be varied, the spiral passage being either given an increasing or decreasing pitch. in accordance with the results which it is desired to secure; for example, if an increased eil'ective force is to be applied in the outer portion of the spiralpassage, for example, to secure a greater force to effect separation of the acid and sludge or heavier liquid outer passage-'way of the spiral, the pitch of the spiral may be decreased toward thecuter margin 4 these conditions, the length of the spiral passageway l2 will be approximatelyY 25 feet and if the depth of the passage is in the order of 4 inches, theI device will be'effective to handle in the order of 500 gallons per minute of oil, assuming a feed of acid of about the amount of oil supplied; that is, about 500 gallons per minute. With a device of these/v dimensions, operated at about 1200 R. P. M., the effective static head of the oil within the rotorapproximates 90 pounds and that of the acid approximates 185 pounds. The

oil is supplied to the rotor .at a pressure in excess of this effective head, suitablyy at a pressure o'f 100 pounds or more and under the conditions set forth, a pressure of supply of the oil" in the order of 100 to 125 pounds has been found desirable.

The substantially greater density of the acid and the resulting larger force with which it is driven outwardly through thespiralpassage causes a rapid and free iiow of the acid with respect to the oil. tributes itself over the inner surface of the out-` side wall of the passage-way in its travel and is intimately contacted at its surface with the oil flowing under pressure in the reverse direction. If desired, as shown with the modified form in Fig. 4, the inner surface ofthe outer wall of the passage-way 20 may be provided with grooves of I any desired form or with other irregularities or projections, so as to cause an internal agitation to v improve or increase the extent of contact between the oil and the acid.

In operation, in the'event of an obstruction or tendency to form an obstruction in the passageway, the heavier liquid `component tends to build up and accumulate back of the obstruction and thereby makes automatically effective a greater increased outward driving force to remove and the power demands for rotation of an apparatus such as that herein set forth are relatively low,.

since the entering light fluid, under the pressure at whichit is supplied, contributes substantially 'to the force effective for rotation of the rotor in thedesired direction.

While the apparatus has been described in connection with specific details of construction and rates of rotation, itis to be understood that these are not essential or critical and that the various factors involved such as the size and rate of rota'- tion of the rotor, the size and pitch of the spiral passage-way andthe spacing of the turns form` ing the spiral passage-way may be varied in accordance with the materials under treatment and the desired result. The rate of rotation is such Vthat the tangential component of the centrifugal force developed, which is effective in securing travel in an outward direction of the heavier component ofthe system is atv a desired value,

`preferably substantiallyin excess of gravity. In

the operation illustrated and described, it is in the order of ten times gravity and in general, I prefer that it shall be not less than two times gravity and preferably at least four times gravity. With liquid components'of the system As pointed out hereinbefore, the aciddis- The device in operation gives a long effectivey path 4for interfacial contact between the components of the system and, as indicated hereinbefore, when desired, by slight groovings or projections'upon the walls of the passage, either for their entire length or preferably in the intermediate pcrtion of the passage alone, some additional agitation or turbulence can be secured, by which even more effective intermingling or coritact of the liquids can be secured. When such groovings or projections are provided in the intermediate portion of the passage-way, the end portions are available for securing a more effective separation of the components near their respective points of discharge while still maintaining interfacialcontact between them.

It is readily apparent that the process and apparatus may be employed for the continuous counter-current treatment of liquids of different Y specific gravities for a variety of purposes; for

traction,` washing or the like. It is likewise apparent that the apparatus disclosed may also be employed for the counter-current treatment of a liquid with a gas or vapor, the latter then following the path of the lighter liquid in the operation as described. Thus, it may be employed in washing of water gas or producer gas or of coke oven gas to remove hydrogen sulphide; for Awashing or contacting gases with lwater or other iiuids to remove fume, solids or the like, and for interaction` between a reactive gas and a liquid, for example, in the chlorination of hydrocarbons. In chlorination or other halogenation'reactions, or in other reactions in which a liquid reaction product is secured from -the reactionof two or more gases,

l the gases intended to react with each other may dislodge the obstruction. It is to be noted that be introduced at the-outlet of the spiral passageway, the liquid reaction product'being discharged therefrom on formation. In lany case,4 such as in the latter reactions,in which the presence of actinic light is desired to effect or aid the reaction, the outer face 21 of the casingll and the outer wall 2?r of the rotor may be constructed in whole or in part of transparent quartz or of a suitable glass or transparent plaster, to permit actinic4 rays from a suitable source (not sho'wn) to enter the passage-way. y

The rotor and other parts in contactwith the materials under treatment may be formed of any suitable chemically resistant material adapted for the intended use; such as glass or quartz; suitable s'tainless steels, such as low chromium and nickel-chromium iron alloys, nickel, Monel metal or the like; or may be plated or vcoated with suitable chemically resistant materials, such as tantalum, platinum, gold, silver, enamel or the like. Various non-reactive plastics of the phenol-formaldehyde or urea-formaldehyde type may also supplying one of said liquids of greater density lto the center of a curved passageway of increas- 2. The method of effecting contact between in- Y completely miscible liquids which comprises supplying one of said liquids of greater density to the center of a curved passage-way of increasing radius, rotating said passage-way to sec're by centrifugal action an outwardly propellant force substantially exceeding that of gravity to propel said liquid through said passage-way, and supplyf ing the lighter of said liquids to the outer end of said passage-way under pressure sufficient to force said lighter liquid inwardly through said passage-way to the center thereof in counter-current contact with said heavier liquids.

3. The method of effecting contact between incompletely miscible liquids which comprises supplying one of said liquids of greater density to the center of a spiral passage-way of rectangular cross-section, rotating said passage-way to secure by centrifugal action an outwardly propellant force to propel said liquid outwardly through said passage-way in a layer adjacent the outer wall thereof, and supplying the lighter of said liquids to the outer end of said passage-way under pressure suiiicient to force said lighter liquid inwardly through said passage-way to the center thereof in counter-current contactv with said heavier liquid.

4. 'I'he method of effecting contact between incompletely miscible liquids which comprises supplying one of said liquids of greater density to the center of a curved passage-way of increasing radius, rotating said passage-way to secure by centrifugal action an outwardly propellant force sulcient to propel said liquid outwardly through said passage-way, supplying the lighter of said liquids to the outer end of said passage-way under pressure sumcient to force said lighter liquid inwardly through said passage-way to the center thereof in counter-current contact with said heavier liquid, and effecting agitation of the heavier liquid in at least part of its travel through said spiral passage-way.

5. The method of effecting contact between incompletely miscible liquids which comprises supplying one of said liquids of greater density to the center of a curved passage-way of increasing radius, rotating said passage-way to secure by centrifugal action an outwardly propellant force suilicient to propel said liquid outwardly through said passage-way, discharging said'liquid into a relatively stationary chamber communicating with the outer end of said passage-way, supplying the lighter of said liquids to said chamber. and maintaining in said chamber a head or pressure of said lighter liquid sufilcient to force said lighter liquid inwardly through said passage-,way to the center thereof in counter-current contact with said heavier' liquid.

6. The method of effecting contact between incmnpletely miscible liquids which comprises supplying one of said liquids of greater density .to the center of a curved passage-way of increasing radius, rotating said passage-way to secure 'by centrifugal action an outwardly propellant force lumcient to propel said liquid outwardly through saidpassage-way, discharging said heavy liquid into a relatively stationary chamber communicating with the outer lend of said passage-way,

y supplying the lighter of said liquids to said chamber,'maintaining in said chamber a head or pressure of said lighter liquid sufficient to force said lighter liquid inwardly through the passage-way to the center lthereof in counter-currentl contact with said heavier liquid, and discharging said lighter liquid centrally from said rotating passage-way.

7. An apparatus for effecting counter-current contact between fluids, a rotor member having a face-plate, a spiral strip mounted on said faceplate, whereby a spiral passage-way is formed thereon, a closurev plate forming an opposing face for said rotor, said closure plate being provided with a spiral groove'into which the edge of said spiral strip is fitted, means for rotating said member, and means for supplying a fluid to the center of said passage-way to be propelled therethrough by centrifugal force resulting from the rotation of said rotor member.

8. An apparatus for effecting counter-current contact between fluids, a rotor member having a face-plate, said face-plate being provided with a central opening, a spiral strip mounted on said face-plate whereby a 'spiral passage-way is formed thereon, a closure plate forming an opposing face for said rotor and closing said passage-way, said closure plate being provided with a spiral groove into which the edge of said spiral is fitted, means for supplying a fluid through the 'central opening of said face-plate to enter the spiral passage-way centrally of the rotor, and means for rotating said rotor member to force said uid outwardly therethrough by centrifugal` force.

9. An apparatus for effecting counter-current contacts between uids, a rotor member having a face-plate, said face-plate being provided with a central opening, a spiral strip mounted on said face-plate whereby a spiral passage-way is formed thereon, a closure plate forming an opposing face for said rotor and closing said passage-way, said closure plate being provided with a spiral groove into which the edge of said spiral is fitted, means for supplying a fluid through the central opening of said face-plate to enter the spiral passage-way centrally of the rotor, means for rotating said rotor member to force said fluid outwardly through the passage-way by the action of centrifugal force, and means for supplying a lighter uid to the outer opening of said passage-way under pressure sufilcient to force it inwardly therethrough. A

10. An apparatus for effecting counter-current contacts between fluids, a rotor member having opposing face-plates, anda spiral strip m/ounted there between, whereby a spiral passageway is formed in sa d rotor, one of said faceplates hav;

ing a central opening communicating with said' `spiral passage-way at the center of the rotor,-

a hollow shaft on which said last-mentioned face-plate is mounted, the central opening in the face-plate communicating with the opening in said hollow shaft, the other of said face-plates being provided with a spiral groove into which the edge of said spiral strip is fitted, means for supplying a' fluid to the center of said spiral passageway, means for rotatingthe hollow shaft, thereby rotating said rotor and forcing said iluld outwardly through the passage-way by centrif` ugal force, means for supplying a lighter fluid to said passage-way at the exterior of the rotor 11. An apparatus for effecting counter-current aoaaeaa under pressure siilcient to force said lighter fluid inwardlythrough said spiral passage-way counter-current to the first-mentioned uid and effecting discharge of said lighter fluid from the center of said passage-way through the opening in said hollow shaft.

contact between iiuids, a rotor member having opposing face-plates and a spiral strip mounted there 4between whereby a spiral passage-way is formed in said rotor, one of said face-plates being provided with a spiral groove into which the edge of said spiral strip is tted, the other of said face-plates having a central opening, a hollow shaft on which the last-mentioned face-plate l is mounted, the opening in said hollow shaft oommunicating through the central opening of said face-plate with the center of the spiral passageway, in the rotor, a stationary pipe extending through the opening in-said hollow shaft and `terminating centrally within the rotor, means for supplying a iluid through said stationary pipe to the interior of said rotor. means for imparting rotary movement to the hollow shaft and the rotor to rotate. said rotor thereby forcing said fluid outwardly through the spiral passage-way in the rotor under centrifugal force developedby the rotation thereof, and means for supplying a lighter fluid under pressure to the exterior of the rotor passedinwardly through the spiral passage-way therein in counter-current to the first-mentioned fluid, said lighter fluid y being discharged through the central opening and the opening in said hollow shaftaround said stationary pipe. Y l

12. An apparatus for effecting counter-current contacts between fluids, a rotor member having opposing face-plates anda spiral strip mounted there between, forming a spiral passageway in said rotor, one of said face-plates'being provided with a spiral groove into which the edge of said spiral strip is fitted, the other of said. face-plates'having a central opening communieating with the center of said passage-way, a hollow shaft on which said rotor is mounted. the

opening of said 4hollow shaft communicating through the central opening of said face-plate with the center of said spiral passage-way, means for supplying aheavy uid at the interior of said spiral passage-way and means for rotating said Vhollow shaft and said rotor to force said fluid .outl' wardly through the passage-way by the action'of centrifugal force, a. casing surrounding said rotor, and means for supplying a lighter `fluid within' said casingunder pressure to cause said lighter..

duid to enter the rotor and travelinwardly throughthe spiral passage therein in counter- -curre'nt contact with the outwardly traveling mst-mentioned fluid, and means for said lighter fluid from the center of sindV sp posing face-plates, a spiralstrip mounted between said face-plates to form a spiral passage- -way in said rotor, means for supplying a uicl within the rotor at the center of said passage-way in said rotor, means for rotating'said rotor to force said fluid to travel outwardly through the passage- 'way under centrifugal force. means for supplying a lighter fluid to said rotor at the outer end of said spiral passage-way under pressure suiiicient to force said lighter fluid to travel inwardly through the said passage-way in counter-current and means for directing active light rays through said transparent face-plate to the interior of said passage-way to induce reaction betweenthe iiuidstherein.

14. The process ofsecuring reaction between fluids which comprises supplying reacting fluids to the interior of a spiral passage-way while maintaining said spiralpassage-way' under rotation to develop centrifugal force suflicient to propel heavier fluids outwardly through said passage-way, at least one wall of said spiral passage-waybeing transparent to active light rays. and directing active light rays against the transparent wall of said passage-way and to the.in

terior thereof to cause reaction between said uids, liquid products resulting from said reaction being forced outwardly through said spiral passage-way.

15. The method of refining hydrocarbon-oils v which comprises supplying an aqueous reactive Vfluid tothe center of a spiral passage-way. rotat- Aing said passage-wayA to secure'by centrifugal action an outwardly propellant force to cause said aqueous reactive fluid to move outwardly drocarbon oil tothe .outer end of said :s: way underpressure suilicient to force l wardly through said passage-way to the center' thereof in counter-current contact: 'with said 4outerjend of said e-wayfunder pressuresufilcient to force said oil inwardly through said e-way to the center thereof in counter-current contact with said sulphuric acid. -l -w samouvto said first-mentioned fluid, at least one face- `plate of said rotor being transparent to light rays,

., through'the passage-way and -supplying the hywsumaarrw 

